参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | Halite (NaCl) | HCID 5234 | — |
| 反应物 | 四氢呋喃 | HCID 8028 | — |
| 反应物 | 1,4-Dioxaspiro(4.6)undec-6-ene | HCID 279481 | — |
| 反应物 | 硼氢化钠 | HCID 4311764 | — |
| 催化剂 | 乙酸汞 | HCID 15337 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 溶剂 | 二甲基对苯二胺二盐酸 | HCID 14798 | — |
| 产物 | 1,4-Dioxaspiro[4.6]undecan-7-ol | HCID 13298811 | — |
反应步骤
Mercury(II) acetate (80.7 g, 0.25 mol) was dissolved in water (150 mL), then tetrahydrofuran (150 mL) was added to give a suspension. To this stirring suspension was added 2-cycloheptenone ethylene ketal (39 g, 0.25 mol). After stirring at ambient temperature for 3 hours, the mixture was cooled in an ice water bath. A 10% aqueous sodium hydroxide solution (150 mL) was added, followed by a solution of sodium borohydride (4.8 g, 0.13 mol) in 10% aqueous sodium hydroxide (150 mL). The mixture was allowed to reach ambient temperature and stirred overnight. The mixture was saturated with sodium chloride, stirred for 30 minutes, then allowed to settle; the solution was decanted into brine and extracted with ethyl acetate, dried over sodium sulfate, filtered, and concentrated in vacuo to give 3-hydroxycycloheptanone ethylene ketal (36 g).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US05723462 |
|---|
| 来源数据集 | uspto-grants-1998_03 |
|---|
| ORD ID | ord-02e021bf3546479584ca183e01838f59 |
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| 来源说明 | uspto-grants-1998_03 |
|---|
